Document K6K8gNrqgmXJJp7VgBLkR7EK0

INC. ESCAMilA PLANT INTEROFFICE MEMORANDUM R. L. Duggan From: L. W. Allen/R. H. Sroufe Re: VCL Emission Test Escambia PVC Plant Date: Copies: 19 October 1978 The VCL emission test was completed on the PVC Plant, and the plant is in compliance. The test was conducted on 17 October as scheduled. Mr. Bill Thomas, Florida Department of Environmental Regulation (Bureau of Air Quality Management) witnessed the test, and Dr. James Wu, EPA, who arrived after testing, reviewed all of the procedures and results. Equipment operating data was taken and is attached. Analytical data for all analyses are also attached. The attached report contains the following. Description of equipment. Conditions during tests. Production calculations, Emission test procedures. Emission test results. LWA-RHS: fls Attachments L, W. Allen/R. H. Sroufe AP00042823 ESCAMBIA BSlLA4UNVT ^ I. PVC THERMAL. OXIDIZER The purpose of the thermal oxidizer Lb to reduce the vinyl chloride monomer discharged to the air below 10 ppm concentration (measured by Method 106). Process gases are purged from the vinyl chloride recovery system. The system consists of compressors and heat exchangers (cooling water, refrigerated water, and freon). On October 17, 1978, the entire heat exchanger system was shut down. This was done to provide an adequate vinyl chloride feed for the thermal oxidizer. Shutting down the heat exchanger system is not standard procedure. This increased the vinyl chloride in the feed composition above normal operating levels, Thermal oxidizer feed samples and flow measurements were taken hourly. The vinyl chloride concentration in the feed increased from 42. 2% to 60. 8%. Mass flow rate of vinyl chloride Increased from 21.76 lbs. peT hour to 34.63 lbs. per hour. Method for Calculation of Vinyl Chloride Feed Flow to the Thermal Oxidizer - Example: Basis. A Gas Chromatographic Analysis was done on feed samples. CO CO 2 CH3C1 Vinyl Chloride 7. 1% 44.9% 1.8% 3.8% .2% 42.2% Specific Gravity of Gas 1.5; Feed Tank Pressure 30 pslg; Ambient Temperature 52F. Principles and Practice of Flow Meter Engineering, by L, K. Spink 9th Edition, Nov. 1975. QN = Cg, Ftf Fg Fpv Fa VhaPf Cg, = Orifice Size = .250" = (17.84) pg 187 Ftf = Fg = Fpv * Fa - Flowing Temperature, pg. 454 (1.008) Specific Gravity, pg. 455 (.8165) Compressibility Factor, pg. 464 (1.026) Temp. Correction on Orifice, pg. 156 (1.000) AP00042824 ESCAMBIA PLANT page 2 I. PVC THERMAL OXIDIZER (cont'd) Qn = (17,84) (1.008) (.8165) (1.026) (1.000) ( -y(20)(44. 7) ) = 450 SCFH pa La PPH SCFH x S. G. = 450 x 1,5 = 51.52 #/hr. of waste gas 13.1 13.1 Vinyl Chloride Flow = 51.52 #/hr. x .422 = 21.74 #/Hr. Thermal Oxidizer Emission Tests The thermal oxidizer was sampled and analyzed on 17 October according to EPA Method 106. The testing began as scheduled at 7:30 a.m. Three samples were taken. During the tests the stack air flow was constant at 202 5CFM according to a pitot manometer. The sample air flow was constant at 1.42 liters per minute to provide an 85 liter sample each hour. The rigid leakproof container and Tedlar sample bags were leak checked prior to and after testing. The equipment was found to be sealed in accordance with Method 106. The gas samples were taken to the lab Immediately after sampling. The samples were protected from sunlight and analyzed within 4 hours. Method 105 was used on all analyses. The test results are detailed below: Thermal Oxidizer Emissions Test Test 1 Test 2 Test 3 Average Sample Time Sample Volume % Oxygen PPM, VC1 1 hour 85 liters 7. 1 None Detected 1 hour 85 liters 6.9 None Detected 1 hour 85 liters 5.5 1. 52 <1.5 ppm The analytical results and operating data of each test run are attached in the Appendix. AP000 -------\ ESCAMBIA PLANT II. NORTH LINE STRIPPER COLUMN- The north line stripper is designed to reduce the vinyl chloride below 400 ppm. concentration in the slurry from the north line reactors, (measured by Method 107). This is accomplished by 40 pound steam flowing up through stripping column and heating the slurry to flash off the vinyl chloride. The vinyl chloride gas Ls then cooled in the overhead condenser. Vent from the condenser is sent to the recovery system. The liquid is sent to the waste water stripping column. During the test period the stripper operated at design rates which are greater than normal permitted rates. Sample Calculation Basis: Operating Conditions During EPA Testing Period - 10/17/78 lb. PYC = Slurry Feed (gpm) x 8.33 lb. x 1. 11 slurry specific gravity x hr. gal. 0.32 lb. PVC x 60 min. lb. slurry hr. lb. PVC = 112 gpm x 8.33 #/gal. x 1. 11 x .32 #/PVC x 60 min/hr. hr. # slurry r= 19; 883.24 #/hr.,rate This translates to an equivalent annual production rate of 174. 2 MM pounds of PVC. The north line rated production capacity is 120 MM pounds of PVC per year. AP00042826 erffo'Phjx&ietl <*W CAemoa& ESCAMBIAA PMLl AANkiTV IMS* II, NORTH LINE STRIPPER COLUMN North Line Stripper Emission Test The north line stripper was sampled and analyzed on 17 October according to EPA Method 107, The testing began as scheduled. Three samples were taken. Prior to sampling, the sample line was completely purged. 60 ml. sample bottles with waxed lined screw tops were used. After sampling the bottles were taken to the lab for immediate analysis. Operating data was collected during the tests and is attached in the appendix. The test results are detailed below. North Line Stripper Column Emissions Teat Sample time Sample volume ppm VCL Test 1 Test 2 Test 3 Average 7:30 a.m. 60 ml 47.9 9:10 a.m. 60 ml 160.2 10:45 a.m. 60 ml 161.2 122.9 ppm The analytical results of each test are attached in the appendix. AP00042827 At -------X ESCAMBIA PLANT <N III. SOUTH LINE STRIPPER COLUMN The south line stripper Is designed to reduce the vinyl chloride concentration in the Blurry from the south line reactors below 400 ppm. (measured by Method 107). This is accomplished by 40 pound steam flowing up through the stripping column and heating the slurry to flash off the vinyl chloride. The vinyl chloride gas is then cooled in the overhead condenser. Vent from the condenser is sent to the recovery system. The liquid is sent to the waste water stripping column. During the test period the stripper operated at design rate which is greater than normal, permitted rates. Sample Calculation Basis: Operating Conditions During EPA Testing Period 10/17/78 Lb. PVC hr. = Slurry Feed (gpm) x 8. 33 lb. x 1. 11 Slurry Specific Gravity x gl* 0.32 lb. PVC x 60 min. lb. slurry hr. Lb. PVC hr. 41 gpm x 8. 33 #/gal. x 1. 11 x 32 #PVC x 60 min. 1# slurry hr. = 7.278. 7 #/hr. This translates to an annual production rate of 63.8 MM pounds of PVC. The south line production capacity is 30 MM pounds of PVC per year. South Line Stripper Emission Test The south line stripper was sampled and analyzed on 17 October according to EPA Method 107. The test began as scheduled at 7:30 a.m. Three samples were taken. Prior to sampling, the sample line was completely purged. 60 ml sample bottles with waxed lined screw tops were used, After sampling, the bottles were taken to the lab for immediate analysis. Operating data was collected during the tests and is attached in the appendix. The test results are detailed below: AP00042828 III. South Lina Stripper Column (continued) South Line Stripper Ernie a ions Test Test 1 Test 2 Test 3 Average Sample Time Sample Volume PPM, VC1 9:25 a.m, 60 ml 21.39 11. 50 a. m. 60 ml 17.55 12.40 p. m. 60 ml 17.70 18.86 ppm The analytical results of each test are attached in the Appendix. AP00042829 ESCAMBIA PLANT IV. WASTE WATER STRIPPING COLUMN The stripping column is designed to strLp vinyL monomer from water streams that contain more than 10 ppm vinyl chloride. Forty pound steam is fed into the column to flash the vinyl chloride out of the water. During the test period the stripper operated at design rate which is greater than normal, permitted production rates. Sample Calculation Basis: Operating Conditions During EPA Testing Period - 10/17/78 Feed (lb. ) = Flow in Gal, x 60 min. hr. min. hr. x 8.33 lb. =20 gal, x 60 min. hr. min. hr. x 8.33 lb;_ = hr. 9,996 lb. hr. Under normal plant operating conditions the column feed is 5, 998 lbs. hr. WASTEWATER STRIPPER EMISSION TEST The wastewater stripper was sampled and analyzed on 17 October according to EPA Method 107. The test began as scheduled at 7:30 a.m. Three samples were taken. The stripper was sampled using 50 ml Hypo-vials sealed with teflon faced Guf-Bond discs. The sample vials were capped with aluminum foil without the discs and muffled at 400C for one hour prior to testing. The sample line was purged and the vials were filled bubble free. The vials were sealed and taken to the lab for immediate analysis. The samples were refrigerated until analyzed. Operating data was collected during the tests and is attached in the Appendix. The test results are detailed below: Waste Water Stripper Emissions Test Test 1 Test 2 Test 3 Average Sample Time Sample Volume PPM, VC1 7.35 a. m. 50 ml 4. 67 9:15 a. m. 50 ml 5.37 10:40 a. m. 50 ml 11.99 7. 34 ppm V. EQUIPMENT AND METHOD USED TO ELIMINATE REACTOR . opening LOSSES Reactors are not being opened on a routine basis. Spray rinse timers have been installed on reactor sight glasses to improve visibility. This improved visibility eliminates the need for opening the reactors when coupled with the established chemical cleaning system. A fill water system exists to fill the reactors completely (100%) with water before chemical cleaning. The vinyl chloride is purged from the reactors to the recovery system. This effectively eliminates the presence of vinyl chloride during chemical cleaning. REACTOR OPENINGS The emissions from reactor openings are essentially zero. The reactors are completely water filled and evacuated prior to openings. Therefore, emission testing is not required. EPA observer. Dr. James Wu, accepted the system of abatement as a procedure. No emissions tests were required. 10/19/78 AP00042831 APPENDIX I. Analytical Data Analytical Log Sheet - Test Results - Method 107 GC Strip Chart Method 107 Integrator Tape Method 106 GC Strip Chart Thermal Oxidizer Feed Analysis II. Equipment Operating Data m North Line Stripper South Line Stripper Wastewater Stripper Thermal Oxidizer AP00042832 ANALYTICAL DATA AP00042833 ANALYTICAL LOG SHEET TEST RESULTS AP00042834 P.V.C . BLURRY AIZ) VENT G.^ RESULTS 3.-TIE I.D. DATE TE-3 A/OAn1 srxt# jVl0+*rT,*r nr fo'n l*-i 7 JOItVfT.pH / jy -)? *iO rrta >r* Vnf* it/ f/^o 3 fij SouT/i r2 jv) j/ V,*A***%Z r h ]? i f-tl it-r> ,>"/ 7 /?-/> /0-t? I/& *c * tl 'f 'TARE TOTAL WT. s;u-t. UT. MfUz. /*-!/7* fi-Zt/r Jl'LUfO nivtr l7'Ziv> /.oitf 1.91.V 7 /.OHS' /e.,ttr* tt,.in / //.flt< /.<9VlS. /4./3.u M.I070 tmrf n.isoC n.iaif n.a&r /7-a.r /, <?/& l, GZ?V 7,0 77/ f.otjf /,3Mf /. /Of TCT/J. SOLUS 'tru' * 7/ij" - 7/0 7 . 7/ry ,/7zf C9i9 SCALING FACTOR <1.** 61/? 2. <>./*- A o,fr M.in r?.iz 61,42- 97/f nr.or POSITION # 7 Sf 9 to ft rz. 'J '4 ir tzs n: < ' r?f ?" ! /r ^ /< ^ tf-uS r eZ /J- fi * nrj. tzz 1 U' 0 0 If/O^ n.-iff z. OT'-i >r COUITS J ppr' VCU 11 i.o i i ;^ iZSSCfl p\ o4V5 / VZs ?f? /yrrr A/?V" V-*7 r-^7 w.z //. 9 7 n.?r /7 7r > j feak i %~ w /.'/*, *. w <=10^ 0 -,r -_ - ---- \/ ___ TIT-OTC? 1 : V. STOP T C i&o T c iC --. j --1---- \/ /\> i ..-TILS T C I'ii 0 '------ j CK-'JII SPIED i /r-*- * ..IT. SETTING i i i 1' range Yib ! -3 PRESSURE J L/3 TEJCP. C --i i i i[ i 1... "" T---- -- \ \ \ . -> .\ -> AP00042835 p.v.c. 9mkbs8 veht g.'lS results -- Thermal....Ox'icH~^ " S-'CTLE I.D. *1 *3. *3 DACE ZT.Z /w; / 7 u!AK TOTAL m. VJT TOTAL SOLIDS SCALING FACTOR PC3UXQH # 7L3 IU 'lilJ. TIME j OOtSrTS i-ta vcm ( 1> ^ H2 AIR f y\\ J A 00 AAk. -Va <:* * 3^ ^ Alt /.ft !if*S'** t/t> r* S y'T .<'* .jL\ J ``3 Ct IOC? ? C Z *> ovr:: t c i' yo s 1 IIIICTOR J l 5 IMJIOTCR 1 T C /% Tw c / f0 i f~ r? S' /> r. /no : `T ' /TO ; va / ft -' > 1 i I 1 i f i \ i c:-:'j.r speed fS !' /5'-- * ah. SE-nuia / RATG2 J LAB PRESSURE ll-` '-t-* -- 1 - <jg rrr^.j) rnO nn r // // <V-C , -U- i > AP00042836 METHOD 107 INTEGRATOR TAPE Column 2 6' x 1/8 SS packed w 0.2% Carbowax 1500 on Carbopack C 800/100 mesh Carrier flow 20 we/min. Chart speed 5 mm/min. Stds. 4190 ppm 1999 ppm 514 ppm 55 ppm AP00042837 AP00042838 &.Wr - 'o'! - - -. v^...- ............... 1Q7 F1UE 1 3 XD lole> id METHOD 3 JLU4j A*c, 1 19 128 1 82 1/ l CAL / ANL AREA ^ 216 2 30 3 7 A 3 263 306168 2 3 >-R. TIME KF CONC "priv. 0108 FILE 1 A xo 1016 ID METHOD 3 1/ 1 CAL / A NL T I ME 127 131 AREA 15Q6A5 127 150772 T I ME KF CQNC 127 7540 19 9 . 9 0 R T 1 MF K F .. f)NC Af ^Ar i 10B FILE ' I 4 XO 1016 10 METHOD 3 1/ 1 CAL / ANL T 1 ME 127 181 area 15064S_ 127 150772 TIME X F CQNC 1 2 7 7540 199 * 9 OR TIME 1i6 127 132 KF CONC 7540 199.90 XF EXP 1 5^ ppW 109 FILE 1 5 XL) 1016 10 method 3 1/ 1 CAL AML TIME 119 128 AREA 317 34017 34334 2 3 TIME KF CONC 126 5600 514 *008 3 AP00042839 -x NJ _ 2 a> -o m >> X Icn w X X O j1to as *- m w K) z m --<t X c o u Ns > r 2> f~ (- tc a O X o Tt -- r ri o -- - O' *-- o vD I I t I w _ u fO N> on M O' mx O' O' * o n o O' >-- *n o O2 oo -x r\. X CD n O' Ce- ?< T1 c O' o o cr 2 co ai o -* *-- -- K> r-- X as NO m ote CJ u> ,w Ph CJ e- X f*N e -J u IS) z n X o CJ *\ \ > ri Z> r r* ai 9 io i tn c. xs X 1 I l AP00042840 1 1HE 95 a </i as x CO -* T> CP T> NJ V) n CO a Zi C P-M --* X c6j O w * \ T| n m \ s. V5 *-* Cl o z r* I- X. - k mi 4 Z a -* M m Cv z CO m X CD m KJ 2. CO cO PI O' Io NJ 1 CD CD oX oo fO 7i ro 7? n ( c Tl . O Tl Tl CO -- VJ 1 o t~ m S) H1* M 1 U1 tr VO cO o oz oo cn o o cz on sc CO ec 1ic*n CO 1* X co PIcD cc w m (O r z r- r- 1c M O t- i I l i AREA 4 10 AP00042841 3 vJ X j cn m > O 3D 0 to rn DO > B CO ~2 PO K> T3 CD Xa m -H 03 I P0, O Xu oo np U) w ' PO Cl \ V ** cn *-- o T] PO > o z> o Ol M a i?i. i in.Bii^niniW TO X aj m o c z r> 03 CD K.' CD 03 CE \o 2 cn rn S CD c> CD 2 OI" 1) cn Is, m ?* -- x -- CX cij] n n u>^ S' s O- .LO -- I CD > CO cn [jo cn & z w cc a> kn -- M r CT1 o o\c? cn O > yin o> PO /> * T1 w 1016 ID NS V r >n z \ 's jpgupw.ii i--i.ui iwy)tp^rw'*.y,l>',,w^ fc V \ 8 o (A) AP00042842 riY V> N AP00042843 METHOD n co \ o > M 1 1 1 1 $ \\J ~4 M SJ x Cj m --i -* mm mm CD tn ro >o X CO cl; SO cn m t o Xk x 1 KJ T1 CO 1 fNJ 1 " mm mm o NO i 'CO > CO CO o sC so z ro rvj o CO >0 O' rcvr]kc> CT c CO z r*i o cr 1*0 w <0 > 33 <o w tv} tt -o l~ O CO > X o> K> * (/> <T> T1 ro X m --t i o o w CO N. S mm >o Z r-- *> f~ B NO CO K O T1 fn mm o M --> tn mm o < N- J cX o^ > C tYo N I I I I AP00042844 l u s i: 5 CP s \ t/i t n w o 2 {-- _rr^ oJ <n \tC ' o $ ro a CD rr x fs *n u> . K> -- O O Z w 03 'O w fr n 1 t> * n -4 1LP > O' O' c O' O' z cn tsi n tol\i CP 03 tn X O- t U> t* 03 m 03 CD MM O' CD > 33 Ur u K> rs.- fv' s *- TJ I CT o o> o V N c to * sO n o j n z > r- r- AP00042845 METHOD o V AP00042846 AP00042847 -j . j t b b(. 5 'fs yj7 #116 FILE 1 12 AO 1UJ6 ID METHOD 3 / 1 CAL 6/ ANL SAmP #1 7163 SP 59.32 1 1H 9A 1 19 us 159 187 AHEA 375 1 429 1 144213 S --mrr~ s 2619 7 149225 TIME KF CGNC 128 7423 161.16 S 161.tie ^Y e' #1 17 file 1 1 3 XQ 1016 10 METHOD 3 / 1 CAL 7/ ANL SAMP 02 ' $F 61,42 n U> 03 > s s n z * r r~ ME THQC X/ >--* _ Nj x co n -w * * N> n U ro ro *o co .-- o 'O X 03 tf n n >o o O vO c z O' O' o * u> O' -- t |o -J W KJ > 5> 00 o > |CD _c fO o >o w-- to NJ f\_> fO a ts> .> z fO *0 O' IP * -n N AP00042848 AK A 447 2582 1 4 5 4 5 -3 T in t 95 119 128 3z -- o< c aa -- 3 s N -- 33 n < -- 11 Q o X w ' UJ r in U. art m r-- Lf> 0. <o (11 X a * O It N C3 < OJ sr CO o x CO UJ 3 lT> r --a r- Oj OL lo a> XI o N <*> < 03 o art (N ai a> a% oo o r Xo rvj in m -- art art art art >-- /V c*> or z<_> r- f9 * 3 in in f-- r-- ** D tL rsj *o Ui 3 T IV -- art i-- P a a _j aJ <Z (_> < art \s o u. v> 00 o CO x> <n Q 3 C7v I Q, art 04 T <t UJ < lO r l/) It AP00042849 METHOD Ob ro o x lA W S&i. \i c\ o \ eS vj; _ K, X C5 m -J u ro *r. CO >-- _ Ob u. rc *-- c X O' <o CD o O' r* -g O *< o oo ro ro r> x to i LP * > -J ro -g ro * <o M F1 fs.' CO r ro <_n CD i> Pmi X m > I {*> l\> AP00042850 & b120 Fl le xo METHOD 3 10)6 ID 1/ 1 CAL / ANL AREA 303142 ' 27 s" 303415 CONC 128 7340 4 1 3. UOfi TIME K F CONC 128 7340 413.00 KF EXP 1 trf- /?fy 121 FILE 1 19X0 101610 METHOD 3 }/ \ CAL / ANL TIME 129 182 AREA 151040 TTb* 151156 TIME KF CONC 129 7560 199.90H TIME KF CONC 129 7560 199.90 KF EXP 1 ^ ]1 2 9 7 b 6 0 v 9 9 0 T lM t KF KF XP 1 2b 79DU B b.C U iU hj *- a: iO h to-b- u b-ltu % ltI -j ffl r1! CT'j-- <_n ]> cj ru 3 m -s X o o w n> n N> 8 tV XU o T) M f -- m for* o M o & Q-- -- --**4 fv 2 CD m UV u 1 o n c t cn 1 --b o G o o Zn --4 -- -- fU CP mz (J1 U) O r O CP to- n o o o33 n2 OJ - Ju 05 >o \C Ca FzI fO K-j! t> > ru 03 o <T> >o mX o -j o> w ro mT X c o co M VV M >n 1z" r>- ro *B-* o tv Ni X O n -- rm c- o> <-* o jJ CoNC 1 AP00042852 THERMAL OXIDIZER FEED ANALYSIS AP00042853 o CO O 33-as 3 0 . 83 3"9 . 05--30 :-ag 40. 23 3eIiT0P EXP RT 30.06 30.33 30.04 30.37 34.32 34.33 40.23 40. 1? XF: AREA 306100 1238000 44320 89400 1.0000 E+ 0 CRL # 7 R1 9 10 RHT 6. 822 0*. 42.955 //+> 1.670 3.625 p 5B30A AREA V. RT 7.96 21.79 25. 17 30.06 30.-83 34.32 39.02 39.05 40.23 BREA Uffl 17i7000 306100 1238000 44320 6693 5980 99400 XF: AREA * 49.601 8.843 35.763 1.280 0. 193 0. 173 2.871 */ V.WH * 0.V ho.J' AT* r >* ^ S A7 * 3> t/6*1 % Sf 8 AP00042854 24.95 092 M 5830ft ESTD " KI 30.05 30.37 34.29 40.25 *-p 5830ft ftREft 7. RT 7.95 21.61 24.95 30. 05 30. 37 34. 29 39.02 KI 30.03 30.97 34.32 40.15 XF: HKtH 301100 1183000 43820 100100 1.0000 E+ CftL # 7 Rt 9 10 rtriT 8.711-^1* 40.353-*,v 1.644-C 3.650<V flRER 16 1 10 1 1010 1879000 301100 1183000 43620 8830 RRER V. 5:Kr-`' 53.284 8.538 32.980 1.237 0.194 VU -*V *f*V -< . r,ttt AP00042855 "~ji *j / o ^wniniouO From Pago _ AP000428S6 fMfi M `' I t! ii -JXgc,mcx\, I Qxidl^^C P.; Sf! } sJ i; ' i ,1 -J'i iFt^i l.l : F''iI'o!tu ; 4 ^>sic^ I oiaI j T^TfTt^ ' z^OO'F; /. Oi*n ! 1j I ; <X \ r; ; '-1 *> H- 1--J -lot--' !^7F! l- ! r ! |V ii i i: -^Cv. rv> Ij |^7 ^ i i . t |< . l\ CA A d r iJc^y] i .il ! ; i 'i i; i rafTti it] -~i.... !j .. ,trv*yiC^\^\^y *>^t*.__oo__tV _ jjFvijJv<uUu)I +^> i - T:h er,*n,a.| O- jTcid1 :.I .*_!i ef\!'r j._Lb_y_______..,C h_c.9 ir <K"tc> ,0. ;^a c* K 4'.lj l. TJi. :.i.j !. i i T i ; o* ; 7. \ % M 1 1! f 4 /o-- +- N z. : 4- ft i ..!.. POi J l.? % . cot i z~ 8 . /o If !i - -I .ilc * Vu v\f 1 j OWlCrtcljc. a> I.I-IS! !. ic/b 1i i1 fK. . ^ipessur? 501 ,<: I : ! j, i J | MJ 'I':; 0^\AF*|o V_) I Co. f tP^JcL V*ro;^j ft, -.j .*. 4 ! A ~c ': . ;'.Onj\7!_~!>-S;*.<cJ; ! ---I j J : Tk-e . I! i | t 1 . 1 ! | j ' i 1 | | i :_1 I /rrf'i Sy'\ /y?*' . i I./&/ ii / T. / /V .T^ .' /v/ / yr j tj -I 1 f i. 1 1 i , 4 r : ; - j , ! *//<-, n ; /'{-//ue.f1'/Ai . jC^.ij ; .!{. I! [.i. | i ' ^ j | /yvt4cii '<>/ / 1/ii'i/W-it A//J; - , l^/ ! l^i. I1 i *; i t l h.i 1. n u 1 )! ,r*- 'm\ ; I ]. TV\c^o_| T ii ! j - -i I .1. i f i . ! ~j! -11 '*//* /?* | _,.j 1 ' i .. ;: T; ! i 1 1 i 1 ; : ; i i A' y 4' ' '. ` 'Am T/--ri' >!_. --f* : 1 ^ u>t i f". T': l^- ' I y,: / 7c*/1' Ij Afr**yy. Wi'.^UiZ. ;' i J j | f . ; ; y/f i it I( ! 4 ( 1 */ , / ^ ! /: ^ : / ^ ; f' j j' | ! : j ; ^ ; / 1| Continued on Pa< IL OIL " ... J*A 4 k r* i y ij rw fj jW t fy AP00042857 ;sct__ ,i n.. 3 r pi bdr* ! Si ` UsZcT*? \ \* f i! i'. c)'n ; : y\ //? 1 {- ' V* / V. .i ' i '+/SO' ^<-/r'T/ ! , 'i . ! ; : * . i ; |- : . //Vi ;; i | I iiii /S-/ t : 'i i ; ;i!: i/^'S'y..ss<r ; f <:/ vc- :. ! ^ : ' . : I _ ! ' ' !_ i ! {/wc')/ Ac*#*'/) i ^ S'-, " .: ` :: .: .:] : ! 1 I ' . ; 'i;,! ! L ; y*o X /S~" J *! :i 'i 1 :[i i a>:/ Yi c'V vj l i, ii \J .J Iv/ft (Ilk** III fU`r* 1 ' - /o/( 7/7 f >. r* /vr ;ty A'//,/Vl AP00042858 1 Co|- t-tx^ ; f ftO SO 5T -- _ / C - i * Tio UC?- ^ + o j f-^<~ Co/- f r^si. -- / 9*& ..... fcp(V o S- ( >> - i> f s' psi'^: p "> / <C: l 1 0 *Q AM -- , j ;.:: ; t ` ^ 4- TeecP P|o w - ^c &?/w c-ti.i- so f-f 0 *>~\ T C. #-n p ' S. 4 ^CL^ 9S'ST^///(V i Co/. O^ Hcc^d? 2*ff * F 0 /6 * ^ /0 i1 J .7/so O V*>. Hr F-j^ '^ &jua>-x^ C < C * ? <^c<^de\ ~ 4-/ TIC - O !ST ( ^7 i-r i ^ f t r ^* Ho^- Z 2. S' S Vr ij ^ r Co lu*v>#i Prsiu. / e - 20 OPR- o^"i.o Co/'- ?rtJb 0 ro ^ (rP^, P ^f^ ^ !>'cl C!Coi rotr r^o 7o-> - z/z.y ^ / A/u AP00042859 f. . 1 m'`'i ri.i -O 9 'bC)c/ ^ - | | F **-ec.J 1 r i C) K.I cjt ^ ec i f fu. U "p(o io f \VCS'\ rh. 'i'1 1 / (X/vi (n t ir " h ( * F ^ ' 0.ar. S-, % j :: /V i --! 2 9. tf 7o CO.-; j/.!/: /- . COL r Is# S' 7ci i ! ! !Me W^/j CJ/v/o - .'!* ?*\. ;o * cl, ^ . -- .GO,;?! /* S- Or., i /- 7 '.. ! I I , 1 !l F9 cJJU, <I; ! V ( cc V ( t1 r\ S -- ;I t lJ 1 ! . : i O A'! x,- /'r/r 'i /,*>A ./'CL. ! !:iI ; :J 'i'ly' i \ 7 : i_\/ ! \/r- ; ' ' 0/-Ma- n~/c ' *,v ( I I ' I V j ! \ ` ' , '' /' In' '/S'S.S>\ ^* i , ': 1 I ; (*' '' ^ - y. /-V.V =. V-J'/s-t? >; / r ! / 'V : 1 ii ' ^C- <{ S\ I i i- t ** /.: r~" s, i/. ^ ''ysf*- :0. 6#s .'tJ'/6- "i I iy*r io nh> ii ' '"it'' I nri Pl*tl" /on AP00042860 |-- - \//ti ^ VK ; |o:'7;i><i S V| S' ^ \ o ?fo i*"-f A 1 CKcv r U /.0^S,iV? : - fc! I l m I tfl 3 200 -....- -...... -- 4_tr4|u----------- . -- k\ .... T 7:1. l \1 Hi 0" -) r.XO'A-'Y,H4o ; vO \ | 1a | A i UvL ,1* TlVr'r ^ fViAn 1 \'/ / 5flirni//iiHMi.. 1 1 V L !. t 40* 140-- 130- 100. ___5LL? '2C9` 10--?tTTrT '20U' ---T--V- I 180-7^V---------f-------------------------------------------- U ^0--------- 180 *>0- :...... --170 A^- -------------./o-/4^ ... C V-> .......... , I- .-! 1 Jt II / --1 60---- -*--I----------f- I 60 ---/ : tv 7 17D- -- LJd 60 ... k i-150 ---------------i---------------->501 r * '*U ....... ! ,, ^ ^J. ............ *v V!^- ~'f 7vocf^,, V \ ^ ^ r> * 7~^:: 8 0 ioo__ iOQ OJSu^ /ofn/yy LtU h^^JL /t/fr/rf AP00042861 S O^vv-^J^-^vfcj \ L^vk-v*^ -- O ~7 Is O ^ o ^ ^ *f fc> (ML /O^l 7^7 f jjvfuA- SjZ/f AP00042862 1 2 -4-0" ! So \ Lbi ' Kio4c S 4" ^ ^ ^ M. V" i\ FkSL-d ^Jv^^ius ^-?^J<l) - **? / T^C-C3 S'7 ac. V ^ *''-' ~ 2 Z S -S t- * i^gec Co (. p r <^s t -- .20 ^ V K -^' 5lo Cel. ^ ti>, bct.^ - 2 - *7 G- P/* F . pS /6w iT Coi . F<* pkm p TA;o7T> - Z ( z .7 i i /ojnjii LiL rb.lfi/n<vJL tefnfrt AP00042863 ^1^40- S+^ \ ^ p id. v* fidJuJ ~ f/C * O 5*1 7 fet V ^*o .-^v - Col- Pros -- ^ V^ u S z, o Col. C^eiv - T *k.Col |OQ* T;^ p 0 70"i> Sfe-- ^idL; l. I' kL03~ foj( 7 j~7 i? ^vtt'^Uv AP00042864 l '--s* i* A^c / -- *s --- 77^e^ :?;** ?wj 1'Jaro T^ .00 3*^5 *UO 3 Vi 5 g'.Z* 3V- *5 gVfc> . SZiil^ /fr*c /%-c^1 /y /Lc -e>5 si 0 *i o *1 o \\5 i/5 -7t> */0 *(d .10 2o *J A>*2-, STfttU- &t<~ T.rt J'.Wo 3'. u*> ?.55> /: o ^ ?io ?:fo ?; <5* 7/^ f/i-5 * 10 .' , /<L Jo ,0@ ,/ -t i- .1 o , / 2it 9 9'.$^ ,J^ / toi"/f(.o A& /*** /? /7 /7 /7 n *&5<j//h II S?a^ /i-r - ?5"/fi' j ;,;:' ._ I '^> | A^; ! Zei^ cX^kJ 17 1 /7 f7 /7 O' n ;i!!1 !i tt'jz//,^ n 17 n 17 n /7 n /7 n 0 ,7 n * / 1 ,. '. !, ,: 1;';: 11'' ;;; :\ =- #5" AP00042865 r /Vc. OA*D< 7^>r G*/7?t*ccO /i^i )lbi : i y^r--- i WHfs \ . ! . ,/*-.'! . - fl S : ! ?;55 ; >>* 1 /p '-'t . : ; : i v/Z- . , : ! : 10\OO, 1 ' #/ ,1 ! />:*" j ; 1 . i | .// i /*:'? I : i ! .! !,/*-* ; I i ! 1 /O'.** ! i.^l : ! ; (6^0 : : ; <*; : ,'5 i te-bf ; 1 : i//2. , i /\ o'.tf? : : ;; i ' , ii ! :- : ! ! >/i'i'tttr > ' l *{ Is, . .... /r-^, :iI: :1 7? '7 . n <7 >7 7? ! n '? '7 n n : '!: ;: .!. ,.; - ;; 1.:1' .ii . '. 1 ; ;,:. ,. n = /.my*-' T^>Ti& ~ /}t<- Z^/ixaS " ZJ> 2s -- fH*<d ( < ' 3 $CJ***1 AP00042866 r In/77 c <_ c * Sftsan ESTD RT 30.tf4 ' 30. *7 34. 29 40.25 *>r 39300 RRER PT 7.95 21.59 24.88 30. 04 30. 37 34.29 39. Q2 39.35 40.25 EXP PT 30.03 ' 30.97 34.72 40.15 xf : RR.ER 247000 84940Q 28020 69020 1.BB00 6 + a CAL * 1 R f 1 9 IB fiRER 1 8090 1 1840 2558000 2470QQ 49400 26020 6804 5586 69020 Q.424 _ .307 8 *' 67.466 frO 6.514 22.402 .739 . 179 a. 147 1.82G RUT 5.5 05 *1- 29.472 (*/%. i. a3b ee 2.31? <.#u O to AP00042867 ' m.i m ' *r t -. "in .1. / ' <U ' UrK i i ' k i*/1 ) i -g '.I ! . ! 1 j / , l_<7- r5./'l/0- \ 1 j s' u ? r /! CttBs** i | t! ^ A$>\ '!ii' T(C. r O S'* 7! .-SiW ! i ! .i I S~'v 1 i CdloLUYij^v M!|!Ii Of ft j- O S'<i.O| IC-fc i. -foilO -- II C 1 i jVc^ ! | r %-rry p *j }* '5 l I; -r-* I T* -i. II .1.1*1 //o r VK * In 4 0. Q. jI . , I1 . f .i { i l: Fe.ec$ slurryi ( lijo !Gi^ic>e| -- i Co|, 1 ei-v. p c.-lo-i 1- ii ' ' ' TR:os:6s H 7 I d . F TRoiSrc *V j- j 7 7l '3, i CF; I ' i I I fT| ! i | sirJ ! i -**.[ Vci ifjiOi F' Vr CSS l-r . /<?. S p><;<X iI '1 CtM* /Q/t7f~zl Jj-cr^ /e/''?/- AP00042868 -1 f <r Ayw '2Jgw^c 3)-Np\>gc -- ' ; i : ! I ; J i i I ' Fe^Jp 2-0 6-^M ; CcA *&* p ^-OfT^ T tCoa p 2. ^ 2 CF - ^7 5" *~/hr : aCo l o> tJ <; h ca. Con (J C/\% e r ' i ;;i;, y^ja. M' PS(-i iI1 9 2,0 A M . i i, K^*v\c_/ ! 0jC (ei (t.?- ./ FvjU Flow, t/cJ? ^k ?-vaaa J fc)tH '2 *4 ^ C?s C F~ S & ivi V $ a. ** CX v s- Sc^ rn p \ I n) W rvdS <J.V -W ft-Y , 3 "3 P ^ Q 6 F* oYlo A ly * i\ f\tv Cx.vcit4^r 7 'ey , G'CX-s e kj C h co r>n I *l > 'T V\ e C fvi Q./ oh Gi <. 9 Vc : AJ z. ^(-7/. c, o r 7 "A- GOc i 3,?Vo /Wt H,n CMof iU -<L ef* V i r\ y\ C. ir\ fo C ic0 *# . 7 /o S.o. L (o , Avi r^/rtP^R/* ftt T7V`P F"o-l( . Flo7v r/c F U if 3 t ps /'cj. f< . P |o xi : L o^lcc V< o *?-> - n. <a. *. F: , p-*^ : AP00042869 ' T 1. , <$' * tty /.' /*/ >; /r tX.i do, * dLjA.s. dV- /-4 r<r * r~t<c^ ,a- i /"y ;: * '*y*c.c.-/pc, /. \zs.iXj y V* */ *>y /~iX *~ j X* t c'l u *. lZc>t c*>? c \>./i C' i/Uw?/- . 3 ` 'ifctrflu, *JC*/ X XL.-K-.t~>. T&V// y s t /4, Qr> - (/^V)(. > ' / r>' V 4k` ,: .: *t XXd y-C .J>'/?f/ ) . f Jv*!U ^ i y AO fy\ s y/> r idV7 t . -/'/?' Ay/ L- .vX </ * ! I ^ aUL . -i 'in r *>h\ AP00042870 R n I} C- TEMPI TIME! RATE TEMP2 TIMES IMJ TEMP TCB TEMP OVEN MPX 60 60 80.0 1.00 90 0.0 60 <60 100 11 90 CHT SPD 0.50 ATTN 2T 6 TCB SGML A SLP SENS a. 35 AREA REJ -- FLOW R 25 FLOW B 132 OPTN 0 0.1 VLV/EXT i:l 7.9 7.9 7.9 . 8.0 1% REJ VLV/EXT VLV/EXT ATTN 2t ZERO 2?! 7 29. 8 39. 0 39. 0 43.0 ?E?9ext- VLV^EXTZERO VLV/EXT VLV/EXTSTOP 1 500 2 3 6 2 W* /&X (D 2 5* '3^^ ->C *0 <** VG^eo t>^ P-AKS CD eo/oa^U ESTB >: RTWs 3 CAL # REF*. 1 2 3 4 5 6 7 8 9 10 11 12 RT 30.97 7.34 9.58 10.37 16; 07 17.51 30.13 33.28 <C4."44 40.29 40.75 41.63 XF: AMT .'AREA 3.4697 E1.3826 E2.3476 E- 2.6813 E- 2.2727 E2.4265 E- 2.2287 E4.8254 E3.7686 E3-6465 E3.1556 E- 2.3689 E- 5 3 5 5 5 5 5 5 5 5 5 5 1.0000 E+ 0 AP0004287I METHOD 107 GC STRIP CHART Chart Speed 5 mm/min. Retention time by integrator is 128-129 sec. AP00042872 I W.i i i { ..S . 1 1 J .i l 1 . i J . I .j i .j F'ERKlIM-fr im1 c : 777 & a:: ZV- a a- yi u; a: a a a' . ' .; ..) i ... ' _tfi AP00042874 AP00042875 ___ L 1 ----- 3s -----$ N T* S ^>. I xy *< ----- ^ ----- f. ."s. >*S. \ *' K____ J Jrj2-sE- ----- V\^ --" V --. O' --L\ ____CO. -..-.-- i-i -- -- --- t ____ 33kj, . -VX- -1^ .) c s ~\r 5------ 3--r ' -'"A > r^= --- J____ __\ ~Xv X "---'sJ. ' _. u ' --O' u- ___u 1 /* 4. t' N;-- s~ ii_*------ .V --- ts /-----kT\ x\ --tV.U*X. ---'------V j-- V -------^------ d-----1 --nr VX Jv Xf\' \------- -- X )\ * * ! 1_1 1 w a" w --V- --r r> _O>s. > `x L sv> --< " 1 -Jl -----VTi NVS--rr^?* --V i---j>-- Xt 1 (VS N/~ V' \'V l ----rX \1 ------- 1-- . ___ ----& -- '-- t ----- ^ v> ---- ^ tV N:-- ii-- 1 1 i K \ -o r wNNl >T NV ---------------- --- b-- --Kf -- ' -- i - _i-- | L-- 1-------------- -------------- 1. 1---------------- ---------------- --- AP00042876 METHOD 106 GC STRIP CHART Chart speed 15 inches/hour Retention time is 3.7 minutes AP00042877 AP00042878 j AP00042879 AP00042880 *I rrniiuuM y>3M `JI?U.VbOddOO 91QU1NOO DiHdVdS `IflldVHS CMC AP00042881 AP00042882